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Laboratory of Hygiene of the State of New Jersey. 



CHEMICAL DEPARTMENT. 



TX 541 
,N5 
Copy 1 



REPORT ON 



The Examination of Foods, Drugs and 

Public Water-supplies C water survey) 



R. O. BROOKS, B.Sc, 

State Chemist. 



Trenton, N. J., May ist, 1903. 



TRENTON N. J.: 
Press of Edwin Fitzgeorge, Cor. Broad and Front Sts. 



OP THE 

U. S. Department of Agriculture. 

Class 



1 



Laboratory of Hygiene of the State of New Jersey. 

CHEMICAL DEPARTMENT. 



REPORT ON 



The Examination of Foods, Drugs and 

Public Water-supplies C water Sumy") 



BY 

R. O. BROOKS, B.Sc. 
Statb Chemist. 




Trknton, N. J., May ist, 1903. 



TRENTON, N. J.: 
Press of Edwin Fitzgeorge, Cor. Broad and Front Sts. 




By transfer 
SEP 2j 1907 



Analytical Data Referring to the Inspection of Foods, 
Drugs and Water Supplies ("Water Survey "). 

By R. O. Brooks, B.Sc, State Chemist. 



The following report deals with the work of the Chemical 
Department of the " Laboratory of Hygiene " of the State of New 
Jersey for the year ending April 30th, 1903. 

Owing to lack of room and equipment in the old laboratory 
at Princeton during the first seven months of the year, very few 
classes of compounds were investigated and the number of samples 
examined was comparatively small, in fact considerably less than 
the number analyzed since occupying our new quarters in Trenton. 
A short description of the latter may not be out of place here. Of 
the four rooms comprising the new "Laboratory of Hygiene," 
three are devoted to chemical work, the fourth, an extra large 
room, being used by the Bacteriological Department for the diag- 
nostic examinations for the physicians of the state. Of the three 
rooms comprising the Chemical Department, one is occupied by 
the analyst of Dairy Products, Mr. Wallace, the other two being 
used for the ' examination of public water-supplies ("Water 
Survey ") and the analysis of Foods and Drugs. The room devoted 
to water-analysis is outfitted with an improved Weston ten-flask 
distillation apparatus, with special sink and glassware cupboard 
nearby, and a special bench with improved Nessler tube comparison 
racks, automatic burettes, etc. The room designed for general 
food and drug analysis is of fair size and outfitted with well-venti- 
lated hood, constant level water-bath, drying oven, balance, polari- 
scope, microscope and other apparatus of a modern analytical 
laboratory. 

In examining foods and drugs, especially for possible prosecu- 
tion purposes, it is very desirable that the methods used be beyond 
criticism, and if possible uniform all over the country. For the 
analysis, of many drugs the "United States Pharmacopoeia" pre- 
scribes certain methods (usually quite reliable) which the analyst 
must use when that book is referred to as the standard. 
That requisition does not preclude supplementary tests however, 
for example, in determining what adulterating oil is present when 
a Pharmacopoeia test shows that some oil is adulterated. For the 
examination of certain foods, provisional "official methods" of 



analysis have been published l)y the "Association of Official Agri- 
cultural Chemists" for use in the various experiment stations and 
these when possible or practicable should be used. Many methods 
of analysis however must be sought out, their reliability proven 
and used as admissable under the circumstances, all of which 
depends more or less upon the judgment of the analyst. It has 
been thought desirable therefore in reporting the various substances 
analyzed to give a brief outline of the method of analysis used, es- 
pecially where there have been prosecutions based upon the results. 
These having stood legal and scientific criticism in our own courts 
may prove of value elsewhere. 

Of the 1476 samples received for analysis, 836 are classed as 
Foods, 616 as Drugs and 24 as Micellaneous. Of these all have 
been analyzed, the following methods having been used and the 
following results obtained. 

FOODS. 
Chocolate mid Cocoa. 

Ten samples of chocolate were received and examined. Six 
of these proved to be of good quality, the fat contents ranging from 

49.3 per cent, to 52.7 per cent, and the alkaloids, theobromine 
(dimethylxanthine) and caffeine (trimethylxanthine) from 1.32 per 
cent, to 1.49 per cent. Microscopical examination showed no 
additions of foreign starches. Of the four samples that proved to 
be adulterated, three showed under the microscope respectively 
about 60, 50 and 15 per cent, foreign starch (corn); fat contents of 

26.4 per cent., 31.7 per cent, and 44.8 per cent, confirming these 
approximations. The fourth sample gave a pronounced test for 
iron, showing the use of considerable ferruginous coloring matter. 
Of the sixty-five samples of cocoa received, eighteen proved to be 
adulterated. Eight of these gave pronounced tests for ferruginous 
coloring matters, while the other ten under the microscope showed 
the presence of foreign starches (wheat and arrow-root) in varying 
quantities, ranging from a mere trace to 35 and 50 per cent! 

Methods of Analysis: Fat. This was estimated by extraction with ''petroleum 
spirit " usinif the Soxhlet apparatus, with fat- free liher-paper thimble and cotton 
plug to hold sample. 

Alkaloids. For estimating the combined theobromine and caffeine, the 
method ot W. Kunze* is used as follows : Boil with 10 per cent, sulphuric acid 
for half an hour, filter and add to filtrate an excess of nitric acid solution of 
sodium phosphomolybdate. After twelve hours standing the precipitate is filtered 



♦Zeitschrift lur Anal. Chemie, Jan., 1901. 



off, washed with dilute sulphuric acid and decomposed with barium hydrate 
solutiou, excess of latter being precipitated with carbon dioxide. Evaporate to 
dryness and extract with boiling chloroform. Upon evaporating the latter the 
alkaloids are obtained perfectly pure. 

Microscopical Examination consists of recognizing the characteristic 
starch granules of various starchy adulterants or the histological structure of other 
known adulterants. A small amount of the sample is moistened and rubbed out 
between slide and cover-glass to a very thin layer. A compound microscope with 
f and G inch objectives and 1 and 2 inch oculars .should be used. A magnitication 
of about 150 diameters is desirable for general appearance of sample, while 250 
diameters is necessary for accurate differentiation of starch granules. For the 
latter also, a polarizing attachment is desirable. 

Coffee. 

Thirt)' samples of ground coffee were received and examined. 
One of the.se was marked "Compound" and contained besides 
coflfee, roasted peas and cereals, being colored with "caramel." 
Seven other samples were adulterated, six with 5 to 15 per cent, 
of chicory and one with peas, chicory, cereals and finely ground 
coal, the latter to the extent of about 12 per cent! Estimations 
of fat, caffeine and ash from the twenty-three samples pronounced 
unadulterated after microscopical examination, supplemented by 
test for starch, gave following results : 



Fat 

Caffeine. 
Ash 



Maximum. I Minimum. 



12.3 per cent. 9.74 per cent. 
137 1.12 

5 04 3.76 



Average. 



10 61 per cent. 
1 263 
42 



These figures are about normal with the exception of the 
maximum percentage of a.sh (5 04 per cent.). This is a trifle high 
and may be due to a little mineral matter not distinguishable under 
the microscope. 

Methods of Ayuilysis: STARCH. Coffee contains no .starch, but many of its 
adulterants do. Test as follows : Boil the ground coffee for a few minutes with 
ten parts of water and set aside. When cold, add some dilute sulphuric acid 
and then strong potassium permanganate solution drop by drop, until color is 
destroyed. Decant off some clear liquid and add iodine solution. Blue or blue- 
black coloration indicates presence of starch. 

Fat. Extract with " petroleum spirit " in Soxhlet apparatus, having pre- 
viously dried the sample to constant weight at 100° C. Extract should be 
between 10 per cent, and 12.5 per cent. 

Caffeine. Boil 6 grams with 600 c. c. water in flask with reflux condenser 
for six hours. Clarify by adding 4 gr. of lead acetate and boiling ten minutes, 
repeating if necessary. Filter, evaporate 500 c. c. (5 gr. coffee) of filtrate to about 
50 c. c, precipitate any lead in solution with sodium phosphate, filter again 
(, washing filter) and evaporate to about 40 c. c. Transfer to separating funnel 



and extract four times with chloroform. Distill off the chloroform from com- 
bined extracts in a tared flask and weigh immediately. 

Ash. This is usually 3.5 to 4. .5 per cent, and rarely, if ever, 5 per cent. It 
is estimated by igniting at a low red-heat, 1 gr. of the pulverized sample, until a 
white or nearly white ash is obtained. A mufile furnace, heated by gas is very 
useful for incinerating purposes. 

Cream of Tartar. 
Eighty samples of "Cream of Tartar" (acid potassium tar- 
trate) were received and analyzed, only ten of which were adulter- 
ated, although a number gave slight tests indicating more or less 
carelessness in its manufacture. Of the ten adulterated samples, 
four contained no cream of tartar at all, three being scientific frauds, 
composed of acid phosphate of lime, alum and flour and yielding. 
when titrated direct with alkali solution, an acid .strength equiva- 
lent to 99 per cent, potassium bitartrate or over. The fourth was 
composed entirely of potassium carbonate and was probably sold 
by the wholesale house by mistake. The other six adulterated 
samples varied, one containing 59.9 per cent, calcium sulphate, 
another 45 per cent, alum, another 64 per cent, flour and the re- 
maining three varying mixtures of acid phosphate of lime, alum, 
flour, and potassium bitartrate (cream of tartar). 

Methods of Analysis : Acid Potassium Tartrate. Test for, by shaking a 
small amount of sample with ammonia in a test-tube, filtering, adding a small 
crystal of silver nitrate and warming. A silver mirror indicates tartaric acid or 
tartrates. Estimate as follows : Ignite 1.88 gr. of sample to fusion in a platinum 
dish, allow to cool, dissolve in water and wash into porcelain casserole or dish. 
Titrate with normal sulphuric acid solution, using methyl-orange as indicator. 
Each cubic centimeter of acid required is quivaleut to 10 per cent, acid potassium 
tartrate. 

Alum. Test for, by mixing some of the sample with an equal quantity of 
sodium carbonate, burning to an ash, exhausting with water, tilteriug and adding 
some ammonium chloride solution. A white tlocculent precipitate (aluminium 
hydrate) indicates alum (aluminum and ammonium sulphate).* 

Phosphates. These are tested Ibr, by adding to a filtered dilute nitric acid 
solution of the sample, a moderate amount of ammonium molybdate test solution 
and gently warming. A bright yellow precipitate indicates phosphates (usually 
acid phosphate of lime). The phosphates and alnm, if present, can be estimated 
by method of K. P. McElroy.f 

Starch is recognized by the blue coloration caused by iodine solution and 
may be estimated by converting it into dextrose, estimating the latter by AUihn's 
method J and multiplying by 0.9. One per cent of starch is equivalent to about 
1.4 per cent, wheat flour. 



*A quantitative method based upon this test, is being investigated and will 
be reported later. 

fBuUetin 13, Part 5, U. S. Department of Agriculture, Division of Chemistry. 
^Bulletin 46, Revised U. S. Department of Agriculture, Division of Chemistry. 



Calcium (" Lime "), is tested for and estimated by precipitation as calcium 
oxalate with ammonium oxalate solution. 

Flavoring Extracts. 

Va7iilla. Fourteen samples of vanilla extract were received 
and examined for strength and purity. Two samples were marked 
"compound, artificially colored" and proved to be alcoholic solu- 
tions of artificial Vanillin and Coumarin (the essential principle of 
the " Tonka bean "), colored with caramel. Three samples not 
marked "compound" proved to be of similar composition also. 
Of the nine samples that were really " extracts" in the true sense of 
the word, five had been made from a mixture of vanilla and Tonka 
beans and contained from .017 per cent, to .147 percent, vanillin, 
and from .012 per cent, to .192 per cent, coumarin. One sample 
contained no vanillin at all. In the four unadulterated samples 
the vanillin ranged from .03 per cent, to .125 percent. There is 
no definite standard for vanillin in vanilla extracts, as the amount 
varies according to the quality of the " beans " used. 

Methods of Analysis : VANILLIN.* Exactly 2 c. c. of the extract are put into 
a test tube and decolorized by addition of freshly-precipitated lead hydrate. It 
is then filtered, the filter being washed well and the filtrate collected in a 50 c. c. 
Nessler tube. ^ A standard solution of vanillin is now prepared by dissolving 
50 milligrams of pure vanillin in 100 c. c. water. 1 c. c. of this solution is 
equivalent to 0.025 per cent, vanillin in sample if 2 c. c. of latter be taken for 
analysis. A series of varying quantities (2, 1, Ij, 2, 2i, 3, 4 and 5 c c.) of the 
vanillin solution in 50 c. c. Nessler tubes and the above filtrate are treated with a 
few drops of bromine water each, and enough of a freshly -prepared 10 per cent, 
ferrous sulphate solution added to get the maximum blue-green coloration in each 
tube. Then by matching the color of the sample tube with proper standard solu- 
tion, by looking at the tubes held side by side against a white translucent surface, 
the percentage of vanillin is determined. 

Coumarin. 25 c. c. are dealcoholized over water-bath and made up to 
original volume with water (non-separation of resin indicates use of alkali in 
manufacture). It is then shaken in a special ether extracting tube with am- 
monia, which forms a compound with vanillin, insoluble in ether, and then ex- 
tracted with four successive portions of ether, drawing off the upper layer each 
time with the adjustable stop-cock tube. The ether extracts are allowed to evap- 
orate spontaneously, the residue dried at 50°C. and weighed as coumarin. 

^ If upon washing, the filtrate becomes turbid, it may be cleared up by addition 
of a drop or nitric acid, without endangering the analysis. 



*Zeitschrift fur Anal. Chemie, 1894. 



Lemon. Niue samples of lemon extract were examined, only 
one of which was up to the required standard, viz.: 5 per cent. 
Lemon Oil and natural color. 

Two samples were marked "compound, artificially colored " 
and contained no lemon oil at all, both being made of " citral " 
and colored with the coal tar dyes, Naphthol Yellow S and Tropaeo- 
lin. In the seven samples not marked "compound," the lemon 
oil present varied from a mere trace (this sample was uncolored) to 
6 per cent. Tw^o of these were above 5 per cent, oil, but in the 
case of one (5.9 percent, oil) Tropaeolin had been used to color it. 

Meihods of Analysis: LEMON Oil. Polarize the extract in a 200 millimeter 
tube at a temperature of about 20°C. The reading, uj)on the caue-sugar scale of 
the polariscope, divided by 3.2 gives the percentage of lemon oil (by volume) in 
the absence of other optically active substances. If cane-sugar has been used to 
facilitate solution of oil, a correction of -.38 in the reading for each 0.1 per cent, 
of sugar found, must be made. 

Coal Tar Colors. To about 25 c. c. of the sample add 10 per cent, 
powdered acid potassium sulphate and heat to boiling. Then drop in a small 
piece of white wool or yarn, previously purified by boiling in dilute alkali solu- 
tion and washing thoroughly, and stir it around for a few minutes. After washing 
in hot water examine the cloth. Natural fruit colors leave the wool practically 
uncolored, while coal tar colors impart a vivid coloration which can be identified 
by supplementary tests. A red coloration upon adding hydrochloric acid to the 
dyed wool (or the extract itself) indicates Tropaeolin. 

Honey. 

Twent3^-seven samples of honey were received and tested, six 
of which were adulterated with "glucose" to the extent of 66.3 
per cent, and 70.3 per cent, in two samples, 42 per cent, in another 
and 10 per cent, to 17 per cent, in the remainder. The two worst 
samples were practically pure "glucose" with a small piece of 
honey-comb to give flavor. The twenty-one pure samples gave 
readings on the cane-sugar scale of the polariscope ranging from 
-6 to -20, the average being -12.9. 

Methods of Analysis: * Dissolve the normal weight for the polariscope em- 
ployed (usually 26.048 gr.) in about 60 c. c. of water, add a little "alumina 
cream " to clarify and make up to 100 c. c. in a graduated flask. Filter and 
take reading in a 200 millimeter tube. A positive reading usually indicates 
"glucose." Estimate the latter by inversion (see under "Maple Syrup") and 
reading taken at 87°C. This reading divided by 1.75 gives the approximate 
percentage of commercial glucose in the sample. 

* Bulletin 65, U. S. Department of Agriculture, Bureau of Chemistry. 



Milk. 
Twenty-eight samples of milk were "analyzed" by the de- 
partment during absences of Mr. Wallace, analyst of " Dairy Pro- 
ducts." Only one of these was found to be below the state stand- 
ard of 12 per cent, total solids, the solids in this case being 10.234 
per cent. The highest percentage was 14.S14, while the average 
was 13.19 per cent. The "anal3^sis" consists of evaporating 10 gr. 
to dryness in a flat-bottomed platinum or nickel dish over a water- 
bath and weighing the residue. 

Maple Syrup. 

Forty-five samples of maple sj'rup were examined for sucrose 
(" cane sugar ") and "glucose," the latter liable to be present as 
an adulterant. These two substances are best determined by means 
of polariscope. A pure maple syrup gives a reading of about 60 
on the " cane sugar " scale. A reading in excess of 65 indicates 
addition of "glucose" without doubt (see method of estimating 
below). Three of the above samples were found to be adulterated 
with " glucose " as follows : 



No. 



Perceutage Sucrose, j Percentage "Glucose." 



37. 
59.5 

58. 



34. 
7.43 
4.6 



Two other samples contained 45.8 per cent, and 44.7 per cent, 
sucrose only. One of these was much fermented, which accounts 
for the deficiency. The other had been diluted without doubt. In 
the forty samples found to be all right the percentage of sucrose 
ranged from 59.1 to 64.2. In twenty of these the direct reading 
(see below) was 63 to 64, the "invert" reading being usually — 18. 
The average percentage of sucrose for the entire 40 samples was 
exactly 62 per cent. 

Methods of Analysis: Sucrose (" Cank Sugar.") Dissolve the normal 
weight for the polariscope employed (usually 26.048 gr.) in about 60 c. c of water 
in a 100 c. c. graduated flask, then clarify by addition of 3 c. c. alumina cream 
and make up to 100 c. c. Filter and fill the 100 millimeter tube of the instrument 
with clear filtrate. Eeading multiplied by 2 gives the "direct polarization" (about 
60 on "cane sugar" scale if syrup be pure). The "invert reading" is now obtained 
by adding 5 c. c. couc. hydrochloiic acid to 50 c. c. of the above filtrate in a small 
flask, heating slowly in water-bath to 68°C, cooling, filtering and polarizing in 100 
millimeter tube, at the same temperature as above, multiplying reading by 2. The 
percentage of sucrose is now obtained by means of the following formula, 



10 

,,_ 100^ D 

wherein S^^percentage of Sucrose, D^algebraic difiference of "direct" and "in- 
vert" polarizations and'_T=temperature at which readings were taken In pure 
maple syrup the percentage of sucrose obtained thua is very close to the first 
("direct") polariscopic reading. If the "direct" reading is appreciably higher, it 
is due to addition of commercial "glucose " The difference or "reading due to 
glucose" maybe utilized for determining "glucose." 

Glucose. *~ The grade of "glucose" used for adulterating molasses, syrups, 
etc has been found to have a polarizing figure always of about 175 (that used 
for jellies, etc., about 150). By means of the following formula : 

"Glucose"=^;^° 

wherein R=' reading due to glucose," a very close approximation of the amount of 
"glucose" present can be obtained. 

Molasses. 

Forty-one samples of molasses were received and examined, 
twenty-two of which were adulterated with "glucose" in quantities 
ranging from 7.9 per cent, to 67.4 per cent. Nineteen of these con- 
tained over 30 per cent, "glucose," thirteen contained over 40 per 
cent., while eight contained 50 per cent, or over. These last were 
practically "glucose" with a little molasses added to give flavor. 

In the nineteen unadulterated samples the percentage of suc- 
rose ranged from 33 per cent, to 51 per cent, as determined by Cler- 
get's method (see above). The average was 44.1 per cent., while 
seventeen gave direct readings between 40° and 50° on cane sugar 
scale of the polariscope. 

3fctho(Js of Analysis : These are the same as for " maple syrup '' except that 
lead subacetate solution is used for clarifying, supplemented by filtration through 
animal charcoal, if necessary. 

Olive Oil. 

In contrast to olive oil obtained from drug stores (see under 
"Drugs,") all except one of the samples from grocery stores, 
twenty-nine in number, were free from adulterants. The majority 
of these were standard brands imported from Bordeaux and Leg- 
horn. The one adulterated sample was composed of cottonseed oil 
entirely. Several samples suspected of containing peanut oil were 
tested for arachidic acid with negative results in each case. 

The specific gravity and "iodine absorption numbers" were 
usually determined, and the U. S. Pharmacopoeia and other tests 



*Leach, 32d report of Mass. State Board of Health (1900). 



11 

applied. The specific gravity ranged from .915 to .919 and the 
" iodine absorption " from 81 to 85.6 per cent. 

3Iethods of Analysis: Specific Gravity. This is determiued with West- 
phal balance or a pycnometer (specific gravity bottle) with inserted ground glass 
thermometer stopper and capillary overflow tube. 

Iodine Absorption Number, (see "Provisional Methods of Food Analy- 
sis ")•* 

U. S. Pharmacopoeia Test. Six gr. of oil thoroughly shaken in test- 
tube with mixture of 1.5 gr. nitric acid and 0.5 c. c. water and heated 15 minutes 
in boiling water, should not become orange or red-brown in color, but should 
retain original pale yellow color, becoming solid upon standing 12 hours at ordi- 
nary temperature. 

Bach's Test. Agitate 5 c. c. sample with 5 c. c. 47 per cent, nitric acid. 
Pale green coloration results. If peanut oil (arachis oil) is present, a pale rose 
color develops. 

Cottonseed Oil Test (Halphen's). Mix equal volumes of carbon di- 
sulphide (containing 1 per cent, sulphur in solution) and amyl alcohol and to 
4 c. c. add 4 c. c. oil sample and heat in bath of boiling brine for 15 minutes. Red 
or orange coloration indicates cottonseed oil. 

Sesame Oil Test (Villavecchia's). Mix by one half minute shaking 
in a test tube 0. 1 c. c. 2 per cent, alcoholic solution of furfurol, 10 c. c. of sample 
and 10 c. c. cone, hydrochloric acid. Crimson lower layer indicates sesame oil. 

Corn Oil Test. Dissolve some of sample in carbon disulphide, add a drop 
of cone, sulphuric acid and allow to stand 24 hours. A violet coloration indicates 
corn oil. 

Preservatives hi Foods. 

Meats. Twelve samples of meats were examined for the pre- 
servatives, boracic acid (or borax), benzoic acid (or benzoates) or 
salicylic acid (or salicylates). Of these, four were found to be 
preserved with boracic acid as follows : sausage meat i, hamburger 
steak 2, potted ham i. 

Sausages. Fifteen samples of sausages were examined for the 
above preservatives. Three were found preserved with boracic 
acid as follows : ordinary sausages 2, bologna sausage i. 

Scrappel. Two samples were examined, one of which was 
preserved with boracic acid. 

Mince-meat. Ten samples were examined for the above-men- 
tioned preservatives, but were found to be free from such. 

B2itter. One sample examined, proved to be free from pre- 
servatives. 

Grape Juice. Six samples examined, proved to be free from 
preservative. 



* Bulletin 65, Bureau of Chemistry, U. S. Dept. of Agriculture, p. 24 to 26. 



12 

• 
Methods of Testing: BoEACic AciD Test. Macerate the sample in water over 
water bath for several hours, filter, evaporate to small bulk, add drop of cone, 
hydrochloric acid and several drops of alcoholic solution of tumeric and evaporate 
to dryness. Pink stain around edge of residue indicates boracic acid. Color of 
residue may obscure pink stain, therefore add drop of ammonia. Blue green stain 
will show if boracic acid be^ present. 

Benzoic Acid Test (^Mohler's).* Make alkaline with sodium hydrate 
solution about 100 gr. of sample, evaporate to a thick mass, acidify with hydroch- 
loric acid, mix with sand and extract in .separating funnel with ether. Allow 
ether to evaporate spontaneously, moisten residue with 2 c. c. sulphuric acid and 
heat until acid vapors escape. Then add a little sodium nitrate gradually until 
liquid becomes colorless. Pour into excess of ammonia and add a drop of am- 
monium sulphide. Red-brown coloration (due to ammonium meta-diamidoben- 
zoic acid) indicates benzoic acid. 

Salicylic Acid Test. Acidulate about 50 gr. of sample with sulphuric 
acid and extract with mixture of equal parts ether and " petroleum-spirit," in a 
separating funnel. Evaporate solvent at gentle heat, dissolve residue in water and 
add a drop of ferric chloride solution. Violet coloration indicates salicylic acid. 

Spices and Condiments . 

Pepper. One hundred and twenty samples of ground pepper 
were received and examined, eighty-eight of which were adulter- 
ated with ground olive stones or nut-shells (cocoanut especially), 
buckwheat, corn, pepper-husks and dust, sand, sweepings, etc. 
The percentage of adulteration varied from a mixture of So per 
cent, ground nut-shells and lo per cent, buckwheat to a sample 
containing only a small amount (5 per cent.) of ground nut-shells. 
The methods for detectingthe.se are entirely microscopical. Several 
authorities have stated that a pepper giving an ash above 6.5 per 
cent, must be considered as adulterated. This is doubtless so, and 
the thirt3'-two samples we found unadulterated by microscopical 
examination gave each an ash less than that figure, the average 
being 5.94 per cent. A low ash however is valueless entirely as a 
judge of the quality of the pepper, as many of the most common 
adulterants yield a very low ash, e. g., 

Ash. 

Buckwheat 2 10 per cen t. 

Walnut shells 1.04 

Cocoanut- shells 0. 54 

Olive-stones 1.61 

Date-stones 1.24 

A high ash suggests the use of pepper-hu.sks (ash 15.61 per 
cent.), cocoa-shells (ash 10.44 per cent.) or dirt containing sand, 

* Bull. Roc. Chim. 1890, 3, 414. 



etc., a conclusion that microscopical examination usually shows 
to be correct. A number of analyses illustrate both of these points: 



Number 


Ash. 


1 


4.4perct 


2 


4.42 


3 


5.24 


4 


8.92 


5 


11.55 



Olive Stoues 
or Nut shells. 

50 per cent. 

30 

40 

trace. 
10 per cent. 



Buckwheat. 

small amount. 
30 per cent. 



Pepper husks 
or Cocoa-shells. 



30 per cent. 
20 per cent. 



Dirt, Sand, etc. 



6 per cent. 



3Iefhods of Analysis: These are almost entirely microscopical (see under 
"cocoa and chocolate"). Olive-stones or nut-shells may be easily recognized 
under the microscope (and often by naked eye) by moistening the sample, spread 
out thin on the microscope slide, with an acid solution of phloroglucol made when 
needed by dissolving about a decigram of phloroglucol in 5 c. c. alcohol and add- 
ing several drops of cone, hydrochloric acid. The ground stones or nut-shells are 
stained a deep carmine, and if present to much extent, give a reddish color to the 
sample layer. 

Ash. This is estimated by igniting (in a well ventilated hood) at a low red 
heat, 1 gr. of pepper until a white ash is obtained . 

Mustard. One hundred and nineteen samples of mustard were 
examined microscopically for starchy adulterants and chemically 
for tumeric. Of this number sixty-one gave pronounced tests for 
tumeric, while forty-one of these showed under the microscope the 
presence of wheat-starch or mustard-hulls (excess), the percentage 
of wheat (approximate) varying from 20 per cent, to 80 percent. 
Twenty-seven samples contained over 30 per c^nt. wheat each and 
of these fifteen showed from 50 to 60 per cent, and .seven from 60 
to 80 p:r cent, wheat. One sample contained about 50 per cent, 
excess of mustard-hulls. 

MeVwds of Analysis : Almost entirely microscopical. After examiniu"' the 
specimen rubbed out thin with water between slide and cover glass to ascertain 
what starch granules are present, it is advantageous to carefully lift up the cover - 
glass, add a drop of 1 per cent, iodine solution and thin out again. By this means 
the starch granules (of which pure mustard contains none) are colored blue and 
the proportion present made easier to decide upon. 

Test for Tumeric. A small amount of the mustard is agitated with 
alcohol in a test-tube and filtered. A piece of filter paper is moistened with the 
filtrate, dried at 100° C and moistened again with a weak solution of boracic acid 
acidulated with hydrochloric acid. Upon drying again a cherry-red color, turned 
blue-green by ammonia, develops if tumeric be present. 

Ginger. Twenty-two samples of pulverized ginger were received 
and examined microscopically for foreign starches, etc. Two sam- 
ples only were found to be adulterated, one containing 60 per cent, 
buckwheat and wheat starch with traces of mustard-hulls and turn- 



14 
eric, and the other containing about 20 per cent, buckwlieat and 
tumeric. 

Cassia. Two samples were received and examined microscopic- 
ally for adulterants but were found to be free from such. 

Cayejine. One sample examined and found to be unadulterated. 

Allspice. One sample examined and found to be unadulterated. 

Cloves. Two samples of powdered cloves were received and ex- 
amined microscopicall)^ for adulterants and chemically to determine 
whether the oil had been removed. The following results show- 
that such was not the case. 



Number. 



Volatile Oil. 



Nonvolatile 
Ether Extract. 



1. 13.5 percent. 7 82 percent. 

2. 16.6 7.4 

Meihods of Analysis; Mostly microscopical (see under "Cocoa"'). 

Volatile and Nonvolatile Ether Extract. Extract 2 grams of the 
powdered material for about 20 hours in Soxhlet apparatus with absolute ether. 
Then allow ether to evaporate off, place the flask containing extract in a dessicator 
and let stand about 24 hours. Weigh as total ether extract. Then heat gradually 
to 100°C. and keep at that temperature for 6 hours and finally to 110° for a short 
time. Weigh again and if weight is constant, the loss is volatile oil and the resi- 
due nonvolatile ether extract. 

Sj/NpS. 

Eleven samples of syrup, not including "maple-syrup," (see 
elsewhere) were examined, all of which were found to be mixtures 
of "glucose" and a little sucrose ("cane-sugar"), the former 
ranging from 27.4 per cent, to 76.7 per cent ! The average percent- 
age of "glucose" for the eleven samples was 56 per cent. Suc- 
rose ranged from 8.9 per cent, to 24 per cent., average 14.25 per 
cent. 

Blethoth of Amilysi.'i : Same as under " maple syrup." 

/ 'inegar. 
One hundred and thirty-four samples of vinegar were received 
and examined for the required state standard and general quality. 
The required standard is at least 4.5 per cent, acidity (acetic acid) 
and at least 2 per cent, solids, if " cider vinegar." This standard 
was attained in fifty-two of the total number of samples received, a 
percentage of about 46 per cent. only. All samples were tested for 
malic acid to determine whether it was "cider vinegar" or not 
and where a positive test was obtained, the ratio of ash to solids 
was also calculated, as a ratio of less than 10 per cent, points to 
addition of unfermented apple material (to furnish test for malic acid 



and increase solids) such as apple pomace, jelly, etc. A ratio of 
less than 6 per cent, is positive evidence that the sample is not 
genuine " cider vinegar."* Nineteen of the eighty-tvi'o samples 
below standard gave no test for malic acid, showing them to be not 
" cider vinegar." Three other samples also gave no test for malic 
acid, but were different from the above nineteen samples inasmuch 
they contained the required amount of solids. These were prob- 
ably " malt vinegars" as the ratio of ash to solids was below 7 per 
cent, and the odor very characteristic. The remaining sixty samples 
proved to be " cider vinegar " by the above combination of tests, 
but were below requirements in acidity or solids, or both, due to 
dilution with water. A number of samples were up to standard in 
solids but quite low in acidity, indicating dilution and reinforcement 
with apple jelly. The highest percentage of solids in genuine cider 
vinegars was 3.314 per cent., while the lowest was .9 per cent. The 
acidity ranged from 7.7 per cent, to 2.15 per cent. Among the 
nineteen samples that were not cider or malt vinegar, the solids 
ranged from .01 per cent, to .764 per cent., while the acidity ranged 
from 2.85 per cent, to 5.2 per cent. 

Methods of Analysis : Acidity (Acetic Acid). This was determined by titrat- 
ing 6 c. c. of sample (diluted with 25 c. C. distilled water), with deciuormal alkali 
solution. The number of cubic centimeters of alkali required divided by 10 gives 
the perceutage of acidity or acetic acid. 

Solids. Ten cubic centimeters (measured by pipette) are evaporated to a 
syrupy consistency in a platinum dish over the water-bath It is then dried in 
an air bath at 100°C for 2^ hours, cooled in dessicator and weighed. 

Ash. The solids obtained above are charred by gentle heat and then heated 
to low redness in a muffle furnace. The charred solids often have a peculiar steel- 
blue color when the sample is genuine "cider vinegar." 

Malic Acid. The absence of this is indicated by adding a little lead acetate 
solution to a few c. c. of the sample. As other substances (molasses, etc.) also 
give a precipitate with lead acetate solution, the formation of a precipitate does 
not necessarily indicate the 2))'esence of malic acid. 

Mineral Acids. The addition of free mineral acids may be detected by 
mixing 5 c. c. of vinegar with 10 c. c. water and adding four or five drops of an 
aqueous solution of methyl violet (1 part methyl violet, 2 B, in 10,000 parts of 
water). A blue or green coloration indicates presence of free mineral acid. 

*Dr. W. Frear, Report of Penn. Dept. of Agriculture, 1898. 



i6 



Summary of Foods. 



Adulterated. 



Chocolate 

Cocoa 

Coffee 

Cream of Tartar 

Vanilla Extract 

Leraon Extract 

Honey 

Milk 

Maple Syrup 

Molasses 

Olive Oil 

Preservatives in Foods. 

a. Meats 

h. Sausages 

c Scrappel 

d. Mince-meat 

e. Butter 

/. Grape-juice 

Pepper 

Mustard 

Ginger 

Cassia 

Cayenne 

Allspice 

Cloves 

Syrups 

Vinegar 



4 
18 

7 
10 



6 

1 

4 

22 

1 

8 

4 

3 

1 







88 

61 

2 









11 

82 



Total 



341 



Not 
Adulterated. 



6 
47 
23 
70 

6 

1 
21 
27 
41 
19 
28 
38 

8 
12 

1 
10 

1 

6 
32 
58 
20 

2 

1 
1 

2 


52 



495 



Percentage of 
Adulteration. 

40. per cent 

27.7 per cent. 

23.3 per cent. 
12 5 per cent. 
57. per cent. 

88.8 per cent. 

22.2 per cent. 
3.6 per cent. 

8 8 per cent. 

53.7 per cent. 
3.4 per cent. 

17.4 per cent. 

33.3 per cent. 

73.3 per cent. 
51.2 per cent. 

9 per cent. 

100. per cent. 
61.2 per cent. 

40.8 per cent. 



DRUGS. 

Acetanilid . 

Six .samples were received and examined for identification ac- 
cording to the U. S. Pharmacopoeia and for unchanged analine by 
the test given below. All six samples were of good quality. 

Test foe Analine by dissolving in cold hydrochloric acid and adding a 
solution of " chloride of lime." A violet coloration indicates presence of analine. 

Acetic Acid. 

Three samples of acetic acid were received and examined for 
the U. S. Pharmacopoeia standard of strength (36 percent, absolute 
acetic acid) and purity. All three proved to be of required purit}^ 
One, however, was deficient in strength, containing only 31 per cent, 
acetic acid. 

Method of Amdyah: The U. S. Pharmacopoeia being a standard recognized 
by the state, it is of course necessary that the tests described therein be used, 
when examining a drug mentioned in that book. Additional tests may be used how. 



17 

ever where it is found desirable or necessary. In examining the above drug the 
Pharmacopoeia tests for presence of lead, copper, snlphuric acid, hydrochloric acid 
or formic acid were applied and Pharmacopoeia method of estimating acetic acid 
used. The latter consists of titrating 6 gr. of sample with normal caustic soda or 
potash solution, using phenolphthalein as indicator. Each c. c. of normal alkali 
required is equivalent to 1 per cent, absolute acetic acid. 

Ammonia Water. 

Two samples of ammonia water were received and tested. One 
was supposed to contain 28 per cent, ammonia gas, but upon 
analysis only showed 21.5 per cent. The other was supposed to 
contain 10 per cent, ammonia gas and analyzed 8 per cent. 
Otherwise they came up to requirements. 

Method of Analysis : Pharmacopoeia tests for metallic impurities, sulphates, 
chlorides and coal tar bases were applied and the percentage of ammonia gas esti- 
mated by titrating 3 54 c. c. with normal sulphuric acid solution, using rosolic 
acid as indicator. Each c c. of acid required is equivalent to 0.5 per cent, am- 
monia gas. 

Camphorated Tincticre of Ophini ( ' ' Paregoric ") . 

Nine samples were received, eight of which were examined for 
methyl alcohol. This substitution was detected in four of the 
samples, when tested as described under tincture of ginger. One 
sample was examined for percentage of morphine. Made as re- 
quired by the Pharmacopoeia, it should contain .052 to .06 gr. 
morphine per 100 c. c. The sample upon analysis gave 0.048 gr. per 
100 c. c, a little below the minimum amount of morphine that 
should be present. 

Method of Analysis : The official morphiometric assay for tincture of opium 
(taking 100 c. c. of sample, but only using one half the usual quantities of ether, 
etc ) was used (see under " tincture of opium ") up to the point of collecting the 
separated morphine on filter paper. Then, instead of trying to weigh the small 
amount obtained, it was treated on the filter with exactly 10 c. c. of decinormal 
sulphuric acid, gradually added, the filter being thoroughly washed afterwards. 
The excess of acid was then titrated with decinormal alkali, using methyl orange 
as indicator. Each c. c. of acid not accounted for by this titration is equivalent 
to 0.0285 gr. anhydrous morphine. 

Castor Oil. 

Eight samples were received and tested for identification and 
presence of "foreign oils" as directed by the U. S. Pharmacopoeia, 
Four samples gave the "test" for "foreign oils" although all other 
indications showed them to be pure castor oil. This "test" is of 
very doubtful value. 



i8 

Chlorinated Lime (" Chloride of Lime "). 

Six samples were received and examined, none of which came 
up to the Pharmacopoeia requirement of 35 per cent, available 
chlorine. The highest percentage found was 26.3 per cent., the 
lowest 16.8 per cent., the average being 21.5 per cent. 

Method of Analysis : The chlorine from 0.354 gr. of sample is liberated in the 
presence of potassium iodide solution and the iodine liberated thereby is titrated 
with deciuormal sodium hyposulphite solution as directed in U. S. Pharma- 
copoeia, page 75. 

Chloro/onn. 

Six samples of chloroform were examined and found to be up 
to Pharmacopoeia requirements, free chlorine, chlorides and pro- 
ducts of decomposition being especially tested for. 
Tests as given in U. S. Pharmacopoeia were applied. 

Cold Cream. 

Five samples of cold cream were examined to ascertain if the 
required oil (expressed oil of almonds) had been used and if not, 
what oil. One sample upon examination showed u.se of cottonseed 
oil, an undesirable practice, considering the singularly bland and 
soothing effects of almond oil. 

Methods of Analysis : The sample is melted by warming gently in a dish or 
beaker over the water-bath and the tests given under "expressed oil of almonds" 
(which see) applied, keeping in liquid condition when necessary, by gently warm- 
ing the test tubes. 

Compound Spirit of Ether. 

Two samples were examined for the 33.7 per cent, (by volume) 
of ether that should be present if the sample be made according to 
the Pharmacopoeia directions. 30 and 32.5 per cent, (by volume) 
was found, indicating that the samples had been made with care. 

Method of Analysis : The ether from 100 c. c. of sample was separated out by 
careful repeated fractional distillation and its volume measured. A negative test 
for alcohol indicated thorough separation. 

Distilled Water. 

In examining samples of what is bought as " distilled water " 
{'' aqnadestillata'') especially for possible prosecution purposes, it 
is imperative that no injustice, due to the peculiar purity require- 
ments for the substance, be committed. We have paid little or no 
attention, therefore, in our analyses to certain impracticable Phar- 



19 

macopoeia requirements, such as absence of " organic matter," car- 
bonic acid or ammonia. These might come from exposure to a 
dusty or vitiated atmosphere or careless corking of " stock bottle." 
A slight mineral residue (silicates) might come from the bottle 
upon very long standing also. When, however, residues often in 
excess of those from most ordinary " tap- waters " are found and 
pronounced tests for chlorides, sulphates, carbonates, calcium salts 
or metallic impurities, which cannot come from glass or atmos- 
phere, are obtained, then it is without doubt ordinary water, and 
to stop such a gross fraud no amount of prosecution can be too 
vigorous. Fifty-seven samples of what purported to be distilled 
water were received and analyzed, only twelve of which were pure 
and only twenty-two of which had any claim to the title "dis- 
tilled water." The residues ranged from 260 parts (!) per million 
to 8 parts, sixteen being above 100 parts and the average being 82 
parts. All samples with the exception of the aforementioned 
twenty-two gave tests for either chlorides, sulphates, calcium salts, 
carbonates or metallic impurities, usually several of these being 
present in one sample. 

Methods of Analysis : Tests were applied as directed in U. S. Pharmacopoeia. 
Residue was determined by evaporating 100 c. c. of sample to dryness in a care- 
fully weighed platinum dish over a water-bath, in a place free from all dust. 

JSiher. 

Seventeen samples of ether were received and examined for 
the Pharmacopoeia requirements of purity and strength. Six of 
these were considerably below the required standard of 96 per cent, 
ether, four containing only 80 per cent. ("U. S. P., 1880, Ether," no 
doubt) while the other two contained 87.5 per cent, and 92 per cent, 
respectively. Several gave tests for aldehydes, had " foreign odor" 
or left residue. One left a residue of 0.014 per cent. Considering 
the simplicity of the ether estimation (see below) there is no excuse 
for druggists selling the old Pharmacopoeia ether. 

Method of Analysis : Teat for aldehydes, " foreign odor " and residue as direc- 
ted in Pharmacopoeia. The percentage of ether is quite accurately arrived at by 
the method therein described, viz : Shake in a glass stoppered 50 c. c. graduated 
cylinder, 20 c. c. of the ether and exactly 20 c. c. of distilled water just previously 
saturated with ether by agitation with pure ether and separation of excess. Upon 
separation of the sample and saturated water, the ethereal layer should measure 
at least 19.8 c. c. showing not less than 96 per cent, ether. From the volume of 
the ethereal layer the approximate percentage can be calculated assuming 19.§ 
C. c, to equal 96 per cent. 



20 

Glycerin . 

Fourteen samples were received and examined for Pharma- 
copoeia requirements, also for minute quantities of arsenic as re- 
vealed by Gutzeit's test (using alcoholic mercuric chloride as indi- 
cator). Three ■ samples gave decisive tests for arsenic when thus 
tested. Seven other samples did not come up to Pharmacopoeia 
requiiements, six of them containing traces of fatty acids, showing 
insufficient purification by the manufacturer. Two of these seven 
samples, including the one free from fatty acids, gave pronounced 
tests for sulphates and calcium (lime) salts. One gave a test for 
lead and all contained " carbonizable matter." 

Tests as given in U. S. Pharmacopoeia were applied. 

Iron and Quinme Citrate. 

Seven samples were received only two of which contained the 
required amount of iron and quinine (14.5 per cent, and 11.5 per 
cent, respectively). Two samples were deficient in both iron and 
quinine, two were deficient in iron alone and one deficient in qui- 
nine. Lowest quinine was 10.714 per cent, the highest 12.5 per 
cent. The four samples low in iron averaged about 13.5 per 
cent, iron, not a serious deficiency. 

3Iethnds of Analysis : Tests for purity as given in Pharmacopoeia vyere ap- 
plied and the iron and quinine determined essentially as described in that vpork. 

Irofi and Strychnine Citrate. 

Two samples were received, neither of which confirmed to the 
Pharmacopoeia standard, viz: 16 per cent, iron and 0.9 to i per cent, 
strychnine. Both contained close to 19 per cent, iron; one, only 
0.693 per cent, of strychnine and the other, what is of course 
more objectionable, i. 413 per cent. (!) of strychnine. 

Method of Analysis : Pharmacopoeia tests for purity were applied and the 
iron and strychnine determined as directed therein. 

Iron Valerianate. 

One sample was received and examined for required iron, 
which should be between 15 and 20 per cent. 19.5 per cent, iron 
was found upon determining the metal as directed under ' ' Ferri 
Valerianas " in the Pharmacopoeia. 



21 



Lead Subacctate Solution. 

Four samples were received and tested for Pharmacopoeia 
standard of purity and strength. One sample contained less (23 
per cent.) than the required 25 per cent, of lead subacetate, the 
other three exactly or a trifle more than what is required. 

Method of Analysis: Pharmacopoeia tests for parity were applied aud the 
lead subacetate determined as directed in that book. 

Lime Water {Solution of Calciitm Hydrate). 

Four samples were received and examined for required per- 
centage of calcium hydrate ("about 0.14 per cent.") as directed in 
Pharmacopoeia. Two were up to standard, one a little below 
(0.1275 psi" cent.), while the remaining one only contained 0.0225 
per cent., or about 15 per cent, of Pharmacopoeia requirements. 

Oil of Almonds {Expressed). 

Forty-four samples were received and examined, only twenty 
of which proved to be pure expressed oil of almonds. Eleven 
samples consisted wholly or in part of the much cheaper substitute, 
sesame oil, twelve samples, of the frequent (and cheaper) substitute, 
peach-kernel oil and one sample of a mixture of sesame and peach- 
kernel oil. 

Method of Analysis: U. R. PHARMACOPOEIA TEST. Two c. c. of the oil is shaken 
vigorously with 1 c. c. fuming nitric acid and 1 c. c. water. Pure almond oil 
forms a white or very pale yellow mixture, which after standing at about 10°C. for 
some hours separates into a white solid mass and scarcely colored liquid. If a 
red, orange or brownish mixture results upon shaking, it indicates adulteration or 
substitution with peach-kernel, apricot, sesame, poppy or cottonseed oil. To deter- 
mine what adulterant has been used, test successive portions for sesame oil and 
cottonseed oil by Villaveccbia's and Halphen's tests (see under "olive oil," 
under " foods ") and for peach-kernei aud apricot oil by the following test : Shake 
five parts sample wiih one part of cold fresh mixture of equal weights of cone, 
sulphuric acid, nitric acid aud water. Immediate orange-red coloration indicates 
peach-kernel or apricot oil. 

Oil of Gaultheria {Oil of Wintergreen) . 

One sample was received and examined to see if artificial oil of 
wintergreen (methyl salicylate) had been substituted. This was 
found to be the case, as the sample had no effect at all upon polar- 
ized light, while the natural oil deviates polarized light a little to 
the left. 



11 

m 
Method of Anahjsix : The 200 millimeter observation tube of the polariscope 
is filled with the oil iiud the two halves of the colored or shaded " field " exactly 
matched. A reading to the left on the scale indicates the natural oil, especially if 
supplemented by a negative chemical test for levulose. If artificial oil, the scale 
reads exactly at zero. 

Olive Oil. 
Fifty-two samples of olive oil from drug stores were received 
and examined, twelve of which consisted wholly or in part of cot- 
tonseed oil and one, wholly or in part, of sesame oil. 

Methods of Analijsis : Pharmacopoeia and supplementary tests were applied, 
as given under olive oil, under ' foods " (which see). 

Phenacetin ( p-Acetamidophenetol ) . 
Two samples were received and tested for acetanilide, the usual 
substitute and unconverted p-amidophenetol, which is poisonous.* 
Neither appeared to be present in either sample. 

Methods of Analysis : Acetanilide Test. 0.5 gr. "phenacetin" is boiled 
with 8 c. c. of water, cooled, filtered and filtrate boiled with a little potassium 
nitrite and dilute nitric acid Then add a solution of mercurous nitrate contain- 
ing a little nitrous acid and boil again. A red color develops if acetanilide be 
present in more than 2 per cent. 

p AMIDOPHENETOL TEST. Melt by gently heating 1.25 gr. crystallized chloral 
hydrate and add 0.25 gr. "phenacetin.'' If red or violet color appears after two 
or three minutes heating on water bath, the sample contains unconverted p amido- 
phenetol. If only a pink color appears after five minutes heating, the sample is 
pure. 

Potassa Solution. 

Four samples were received and examined for required per- 
centage of caustic potash, w^hich is "about 5 per cent." One 
sample only contained this amount, the other three containing 4.3 
per cent., 4.2 per cent, and 2.52 per cent., the last being only about 
half the required strength. 

Method of Analysis : Pharmacopoeia tests for purity were applied and alkali 
determined by titration with normal sulphuric acid solution as directed therein. 

Potassium Arsenite Solution {^'Fowler'' s Sohition "). 

Five samples were received and examined for the required 
amount of "arsenic" (arsenous acid), viz : i gram in 100 c. c. of 
solution. None of the samples contained this amount however, the 
nearest approach to it being .98 gr. The other four ranged from 
0.89 to 0.8 gr. per 100 c. c, 

*Allen'8 " Commercial Organic Analysis" III., 2 p. 83. 



23 

Method of Analysis : Arsenoua acid is determined as directed by Pharma- 
copoeia, by titration with deci-normal iodine solution. 

Potasshim Bitartrate {Cream of Tartar.) 

Eighteen samples of potassium bitartrate from drug stores 
were received only one of which could be called adulterated and 
that only to the extent of 5 per cent, starch. A number of samples 
to be sure contained traces of chlorides, sulphates or calcium salts, 
which are contrary to the strict Pharmacopoeia requirements, yet 
when we consider that the percentage of bitartrate in no sample 
was less than 99.5 per cent, and on the average nearly 99.8 per 
cent., it is evident that a great improvement over the former quality 
of this drug exists. 

Methods of Anali/sis: Pharmacopoeia tests for purity are applied and the bi- 
tartrate determined as under " cream of tartar," under " foods." A blue color 
with iodine solution indicates addition of starch. 

Qziinine Pills (2 a7id j grains) . 

Twelve samples of 2 grain pills and one sample of 3 grain pills 
were received and examined for the professed standard of quinine. 
Three samples contained the stated amount of quinine, the other 
ten including the 3 grain pills, being below standard. The amount 
of quinine varied from 2.85 grains (from the 3 grain sample) to 1.62 
grains, the average for the twelve 2 grain samples being 1.87 grains. 

Method of Analysis: Dissolve one pill in 20 c. c. water by heating on water- 
bath, renewing w ater if necessary. Transfer with rinsings to separating funnel, 
allow to cool, add 5 c. c. cone, ammonia and shake. Now extract the precipitated 
quinine with three successive portions of chloroform of 10 c. c. each, allow com- 
bined chloroformic extracts to evaporate spontaneously in a weighed platinum 
dish, dry at 125°C for several hours and weigh as anhydrous quinine. 324 parts 
of this is equivalent to 378 parts of " U. S. P. Quinine." 

Quinine Sulphate. 

One sample was received and upon examination was found to 
fulfill the Pharmacopoeia requirements of purity. 

Soda Solution. 
One sample was received and examined for the required 5 per 
cent, of caustic soda and found to contain just that amount, when 
tested as directed in the Pharmacopoeia. 



n 



m 
Spirit of Nitrous Ether ( ' ' Sweet Spirits of Nitre " ) . 

One sample received and analyzed and found to contain the 
" about 4 percent, of ethyl nitrite" that should be present. This is 
estimated by determining the volume of nitrogen dioxide evolved 
in the nitrometer as directed under ' ' Spiritus Aetheris Nitrosi ' ' in 
U. S. Pharmacopoeia. One other sample contained 3.2 per cent, 
ethyl nitrite. 

spirits of Caviphor. 

Seven samples were received and tested for methyl alcohol and 
roughly, as to the percentage of camphor, which should be 10 per 
cent. Four samples contained less than that amount, three con- 
taining only 5 per cent, or less. One sample gave a test for methyl 
alcohol, when tested as described under tincture of ginger. 

Camphor was determiued (roughly) by adding excess of water to 10 c. c. of 
the sample and after filtering off the precipitated camphor, drying in a rapid cur- 
rent of air and weighing immediately. 

Tartaric Acid. 

Three samples were received and examined for Pharmacopoeia 
standard of purity and strength and found to be up to all require- 
ments. 

Tincture of Ferric Chloride. 

Thirty-eight samples of tincture of ferric chloride were received 
and examined for the percentage of iron required by the Pharma- 
copoeia, viz: "abovit 4.7 per cent." Nine were found to contain less 
than that percentage of iron, the lowest being 3.15 per cent., the 
average being 4.03 per cent. Ten were found to contain exactly 
4.7 per cent, iron, showing considerable care in its preparation 
(more so in fact than many of the more dangerous or powerful tinc- 
tures) and nineteen contained more than the required amount, the 
highest being 8 per cent. (!) the average 5.5 per cent. Several 
samples contained traces of other metals. 

3Ietho(l of Analysis : Pharmacopoeia tests for purity were applied and the 
iron determiued hy titration as directed therein. 

Tincture (" Essence'") of Ginger. 

Eleven samples were received and tested for methyl alcohol 
(" wood alcohol "). Four samples gave positive tests with the 
following modification of Mulliken and Scudder's test.* 

*American Chemical Journal, 1899, 21, 266. 



25 

Test for Methyl Alcohol, Put about 100 c. c. of the sample in a small 
flask and distil off about 10 c. c. keeping the temperature below 70°C. Oxidize 
the distillate by putting it in a test-tube and plunging a red-hot roll of copper 
gauze, oxidized by heating a moment in the oxidizing flame of Bun sen burner, 
into it (the test-tube only) several times. Allow to cool and test contents of tube 
for formaldehyde by adding to pure milk, adding a few c ca. of hydrochloric acid 
containing a trace of ferric chloride and gently heating, rotating the dish mean- 
while to break up the curd.* A positive test for formaldehyde indicates use of 
methyl alcohol in preparing the tincture. 

Tincture of Iodine. 

One hundred and forty-six samples of tincture of iodine were 
received and examined for the required amount of iodine, viz : "7 
grams per 100 c. c." Twenty-six only (!) were up to or above 
standard, five of these being nearly saturated solutions containing 
about ID gr. per 100 c. c, the average of the other twenty-one 
being 7.5 gr. per 100 c. c. The hundred and twenty samples below 
standard ranged from 6.8 gr. down to only 0.6 of a gram (I) five 
containing less than 2 gr. per 100 c. c. and twenty containing less 
than 4.5 gr. per 100 c. c. The hundred samples containing between 
4.5 gr. and 7 gr. averaged 5.49 gr. per 100 c. c. The average for 
the whole one hundred and forty-six samples is only 5.34 gr. per 
100 c. c. Several of the poorer samples were made up with " wood- 
alcohol." 

Method of Analysi>< : 6.3 c. c. of the tincture is mixed with a solution of 2 
grams of potassium iodide in 25 c. c. distilled water and titrated with deci-normal 
sodium hyposulphite solution using starch solution as indicator. Each c. c. of 
the hyposulphite solution required is equivalent to 0.2 gr. iodine. 

Tincture of Niix Vomica. 

Thirteen samples were received and examined for the required 
amount of combined alkaloids ("brucine and strychnine"), viz : 0.3 
gr. per 100 c. c. Six contained this amount, while only two of the 
other seven were very much below, the extremes being 0.1274 g''- 
and 0.327 gr., with an average of 0.2884 gr. per 100 c. c. for all 
thirteen samples. This shows commendable care in the preparation 
of this powerful drug as of course should be the case. 

Method of Analysis : 100 c. c. are evaporated to dryness over a water-bath 
and the residue assayed by the process given under '' Extractum Nucis VomiciB " 
in the U. H. Pharmacopoeia. The percentage thus found multiplied by 0.02 gives 
the weight in grams. 



*Leach, 29th Report of Mass. Board of Health, 1897, p. 558. 



26 



Tincture of Opium (" Laudanum "). 

One hundred and one samples were received and examined for 
the required amount of cr3^stallized morphine, viz: 1.3 gr. to 1.5 
gr. per 100 c. c. Twenty-four samples only were up to or above 
the minimum requirement, two containing 1567 gr. and 1.593 g^, 
respectively. The seventy-seven samples below the minimum re- 
quirement ranged from 1.29 gr. to only 0.313 gr. ( !) per 100 c. c, 
thirty-five containing less than i. gr. per 100 c. c. The average 
for the whole one hundred and one samples was 1.0353 g^^- P^^^ 
100 c. c. 

Method of Analysis : The U. S. Pharmacopoeia morphiometric assay method 
for tiucture of opium (" Tinctura Opii ") was followed, no other method being ac- 
ceptable in the state courts. 

SUMMARY OF DRUGS. 



Acetanilid 

Acetic Acid 

Ammonia Water 

Camphorated Tincture Opium.. 

Chlorinated Lime 

Chloroform 

Cold Cream 

Castor Oil 

Compound Spirit of Ether 

Distilled Water 

Ether 

Glycerin 

Iron and Quinine Citrate 

Iron and Strychnine Citrate 

Iron Valerinate 

Lead Subacetate Solution 

Lime Water 

Oil of Almonds (expressed) 

Oil of Wiutergreen 

Olive Oil 

Phenacetin 

Potash Solu tion 

Polassium Arsenite Solution — 

Potassium Bitar trate 

Powdered Opium 

Quinine Pills 

Quinine Sulphate 

Soda Solution 

Spirit of Nitrous Ether 

Spirits of Camphor 

Tartaric Acid 

Tincture of Ferric Chloride 

Tincture (," Essence ") Uinger 

Tincture of Iodine 

Tincture of Nux Vomica 

Tincture of Opium 

Totals 



Adulterated. 




1 
2 
5 
6 

1 
4 


45 
6 

10 
5 
2 

1 
2 

24 
1 

13 

3 
5 
1 


10 



1 

5 

9 

4 
120 

7. 
77 



370 



Not 

Adulterated. 



6 
2 

4 

6 
4 
4 
2 

12 

11 
4 
2 

1 
3 
2 

20 


39 
2 
1 


17 
1 
3 
1 
1 
1 
2 
3 

29 
7 

26 
6 

24 



246 



Percentage of 
Adulteration. 



55.5 per cent. 

79.0 per cent. 

35.3 per cent. 
71 4 per cent. 

71.4 per cent. 

54.5 per cent. 
25.0 per cent. 

5.5 per cent. 
77.0 per cent. 

71.4 per cent. 

24.0 per cent. 
36.3 per cent. 
82.2 per cent. 
53.9 per cent. 
76.2 per cent. 

60 .0 per cent. 



27 

MISCELLANEOUS. 

Beef Extract. One sample was examined for suspected 
" glucose," but was found to be free from such, the reducing action 
upon Fehling's solution, which had caused the physician to suspect 
it, being due to certain extractives from meat, probably creatine. 

Brandy Drops. Three samples were examined for the percen- 
tage of alcohol contained in the syrup, according to method des- 
cribed by Leach. 1.65 per cent, alcohol was found in one sample, 
.27 and .34 per cent, in the others. 

Ca7idy {''Yankee Grab Package''^). A penny package of bril- 
liant pink and yellow pieces of sugar candy. Examination showed 
presence of the coal-tar colors "Eosin" and "Naphthol Yellow S." 
the former in great excess. One small piece of candy dyed several 
yards of woolen yarn a bright pink. 

Cajiued Beans. One sample was examined for poisonous 
metals (especially copper, for coloring purposes), but none was 
found. 

" Cream Albumenoid.''^ Sold as dessicated milk solids for use 
in thickening cream. Analj'sis showed it to be simply a mixture 
of pulverized gelatine, boracic acid and flour. 

Dye for Colorijig Sausages. This proved to be an impure 
sample of the sulphouated coal-tar color "methyl-orange." For 
its physiological effects upon pancreatic digestion, see Weber in 
"Journal of American Chemical Society," 18, 1092. 

Extract of Sarsaparilla {Beechent s). Solids 1.23 per cent., 
alcohol I.I I per cent. No standard claimed, therefore no criticism 
possible. 

Linseed Oil. One sample, upon examination (by determining 
"saponification number" and specific gravity), proved to be "boiled 
linseed oil " of good quality. 

Prepared Milk. One sample examined for harmful ingredi- 
ents, but none found. 

Egg Powder. One sample of dessicated ^%% for bakers' use 
was received and examined for genuineness and use of coloring 
matter and preservatives. A determination of the percentages of 
protein (43.2 per cent.) and fat (34.8) showed it to be an &%% pro- 
duct without doubt. It was extensively colored with tropaeolin (a 
coal tar color) however and was preserved with salicylic acid. 

" Vanilla Crystals.'^ One .sample of Butler's "Vanilla Cr)'stals" 
was received and examined. Analysis showed it to be granulated 



28 



^ 



sugar containing .043 percent, vanillin and .027 per cent, coumarin, 
having a value of less than i cent. 

Evaporated Cream. One sample examined for preservative and 
found free from it. 

Salad Oil. This was an oil sold by mistake and the cause of 
sickness "diagnosed" as "arsenical poisoning." Examination 
showed it to be lubricating oil, free from arsenic. 

''Shaker Sail." Two samples of prepared salt, which upon 
analysis proved to be identical, containing 98.5 per cent, sodium 
chloride, i per cent, calcium carbonate and .25 per cent, calcium 
sulphate. 

''Catarrh Cure." One sample, 2^ per cent, cocaine claimed, 
2.1 percent, found. 

Mineral Waters. Five samples of well known mineral waters 
(Apollinaris, Vichy Celestin, Saratoga Vichy and Saratoga Kissin- 
gen and Poland Spring) were examined for principal mineral con- 
tents and found to agree moderately close to published analyses 
of same. Strictly speaking, the last brand (Poland Spring) is not a 
mineral water, but simply a quite pure spring water. 

Suspected Well-ivater. A well water " suspected of containing 
arsenic." No arsenic found. Chlorine rather high however (27 
parts per million) indicating possible pollution from house drainage. 

Total Summary. 



Foods..". 

Drugs 

Miscellaneous . 



Totals 



Adulterated. 



341 
370 

7 



718 



Not 
Adulterated. 



495 

246 

17 



r58 



Percentage of 
Adulteration. 



40.8 per cent. 

60.0 per cent. 

29.1 per cent. 



48.6 per cent. 



" WATER SURVEY." 

This is intended to be in time, a systematic periodical examina- 
tion of the public-water supplies of the state for advisory and, if 
necessary, legal purposes. Several examinations will be made 
yearly and such suspected private supplies as reach the laboratory 
through the proper authorities will be analyzed also. Only a few 
examinations have been made as yet, and it is very doubtful if a 
respectable showing can be made, in addition to the food and drug 
inspection, with a laboratory force of one chemist only. 

The analyses up to date are as follows, with results in parts 
per million : 



29 






■ if JUJO 

l^J^ox 



•saiBiiijyi 



OiOOOOOOO 
0010t00j>00 



"sa^inj^ 






I cj 00 ;o 



OO oOOOMO 
OOjgoOOrlO 



o o o 
o o CJ 

eC 00 rH 



CO (N O Tj< M tH 
O tH O CO o o 
O O O OO o 



o o 
o o 

00 T-l 



;z;^ 



•anuoiqo 



lOcoco-^t'-^iOLo'incoodoi^'r-HTHtooi-J-rtSj^; 



•pioni 
-ninq^V 



•98.IJ 



C0'MC0(M<Ml^«55OOSt^i-lM<f0 

OOOC<(OOCOOMiOOOO 



•Aipiqanx 






li 



a -^ 



e3 a 




•spiiog 

mox 


OI>-0-^-*rH-^T-(OOOmOOOOQOOO«0 

l-H r-l (M a C^ y-i 7-^ 0(M •<*l 



tJD 



q g _a 






L=o 



^ {3 ce CD (» 

cS k 



^ a 



<4^ •)-l 













•laqran^ 



i-l(MM';fin=Ct-00MHH^SKSM><i!:1tHS 



I / / 



30 

COURT ATTENDANCE. 

In addition to the foregoing analytical work and the design- 
ing, outfitting of, and moving into a new laboratory, there has 
been furnished expert evidence for eighty-nine (89) prosecutions as 
follows: Cocoa (4), cream of tartar (5), maple S5'rup (i), milk 
(i), molasses (2), mustard (9), pepper (13), vinegar (6), almond 
oil (10), distilled water (9), olive oil (6), tincture of iodine (9"* and 
tincture of opium (14). In the majority of these personal attend- 
ance was required at court and adjournment frequently necessi- 
tated a second or third attendance. Conviction resulted in seventy- 
four (74) cases, one was appealed, six are pending, six were with- 
drawn and two lost on legal technicalities concerning the collection 
of the sample. 



LIBRftRY OF CONGRESS 



014 338 243 6 ^ 



